Co1-xFex-HPAA metal phosphonates were prepared and pyrolyzed under N2 and H2/Ar flows. The resulting powders were structural and electrochemically characterized by XRD and CV, respectively. The obtained materials possess different structures depending on the temperature and pyrolysis atmosphere. Samples pyrolized in N2 at 1000 ºC are monophasic diphosphates, while
phosphides form in H2/Ar at 850 ºC.